Chemical apparatus



W. H. MAHLEB. CHEMICAL APPARATUS.

APPLICATION m'so MAY 25. 1918. RENEWED APR. 26. 1921.

1 ,4 O5,733, Patented Feb. 7, 1 92 2.

I I 141-11 [III/7,774

38, A!) arrow? "UNITED STATES PATENT TOFFlCIEZELQc WILLIAM MAHLEB, OF NEWARK, NEW JERSEY,

CHEMICAL APPARATUS.

Specification of Letters Patent. Patented Feb, "7, 1922,

- Application -fi1ed May 25 1918, Serial no. 236,512. Renewed April 2e, 1921. seriaruo. 404,535;

To all whom ii may concern:

Be it known that I, WVILLIAM H. MAHLER,

a citizen of the United States, residing at Newark, county ofEsseX, State of New J ersey,ohave invented certain new and useful Improvements in Chemical Apparatus, of which the following is a specification.

This invention relates to chemical apparatus. I

More particularly thisinvent on relates to chemical apparatus for effecting the hydrogenation or reduction of organic compounds for deriving benzidine from nitrobenzol or its homologues. V

A preferred form of my invention comprises a movable container provided with suitable mounting means, and having a charging and discharging opening, provided with a liquid-tight closure, shelves arranged interiorly of the movablecontainerand ex tending more or less transversely to the direction of movement of the movable con tainer, and agitating means movable upon the movement of the movable container and extending more, interiorly thereof relatively to the shelves. In the mostpreferred form of my invent-ion, the movable container is a cylindrical drum, mounted in bearingsto be rotated. A; discharge piping for removing the gases ensuing in the treatment may be provided, extending through one of" the bearings. A recording thermometer preferably of the pyrometer type, is arranged to indicate the progress and termination of the respective stages ofithe treatment. I V

Other features and objects of the invention willbe more fully understood from the following description and the accompanying drawings, in WlllCll F ig. 1 is a central vertical'section of on form of my invention; and

Fig. 2 is a transverse section on the line steel or the like, is provided at a circular extend-more than one-third of the vertical trunnion 7 mounted in the-bearing 9,'the

open end of the trunnion communicating in gas-tight relation with the gas exhaust pas sage 10', discharging as desired, into a flue, V washer or the like. The bearings of the axisf'of the drum 1. shelves 11 are arrangeda'pluralityof open- At the opposite circular end 6 of'the drum 1 may be provided the h'ollow yp c Interiorly; of the drum are'arranged the" I shelves 11 extending more orless radially, said shelves llbeing fixedonthe inner part substantially in planes passing through the '60 Goacting with said N faced agitating 7 members 12- extending;-

toward the axis of the drum more interiorly ascompared with the shelves 11.- VThe' shelves 11 may be perforated,- ifdesired;

Preferably, the agitating 'members 12' are.

disposed in sets or series 'afli'xedto-the :re-

spective shelves 11 and preferably'in zigzag :or staggered relation to oneanother. Thus, in the drawings, I have'indicated ailternate setsv of'two and three members ex tending. radially with respect to the. suc:-'. cessive shelves, the number-of membersin' the respective setsibeing chosen in "accord ance-with' the desired degree of'agitation.

' The indicator 13is connectedby suitable circuit leads 14 with the pyrometer 15 pos1-- tioned within the drum 1. lnmy-co-pending" application Serial Number 236,511, filed by me on- Ma-y 25, 1918, entitled Methodof deriving benzidine andits' homologues, I' have set forth a new'anduseful method of" deriving benzidme or itshom'ologues, :b

charging an aqueous mixture of nitrobenzof,

caustic soda and zinc in either; granular, 1

flake or feather form. r The: proportional: parts of the aforesaid ingredients by weighttl" are, in the order named, 123, 50: and-200,

with approximately 300 parts by weight of water. r

The water may be first charged, then the caustic soda is added; then the nitrobenzol is poured in: and finally: the full amountr'of zinc in granular," flake or feather form is charged, preferably distributing the -'zinc a as uniformly as possible on the bottom, of:

the interior of the drum.

height of the drum: r

The entire chargershould, preferably-duct The charging ismade'through the opening I 18, which is provided with the gasand liquid-tight closure 19.-

vThe drum is now rotated suitable. driv ing means, at a speed of say'from 15 to 20- R. P. M; The reaction ofthe-zinc particles and the caustic soda results in the gradual and continuous evolution of nascent hydrogen, with the development of heat of sufiicient amount to provide for its own reaction temperature, without any supplemental heat supplying means.

The proportional yield is increased by V coating the drum with asbestos or like heat insulating material, and, also, by enclosing the whole a paratus in a wooden housing. The rot'atlon of the drum continuously raises the. zinc in the direction of rotation and also the heavier contents of the charge,

which drop back into the mass, continuously repeating the thorough agitation of all portions of the mass as the drum rotates.

The complete reduction or hydrogenation of the nitrobenzol takes place in a period of from fourteen to eighteen hours, and personal attention to the apparatus or for feedingthe zinc or other ingredient of the charge is'entirelyeliminated. The indicator card shows by a fall of temperature, say below I 50 C. when the reaction has been completed.

'The'ev'olved gases are conducted through the piping 10 to the atmosphere or through a-washer, or otherwise. 7

A particularadvantage of my invention is'the thorough agitation "or circulation throughout the reaction period of the whole of the charge, enabling the whole zinc content ofthe charge to be fed in at one time;

also, in rendering possiblethe use of granular or flake or feather, zinc instead of zinc dust, as necessitated in accordance with prior proposals. The attendance of an operator is obviated entirely, after charging and initiating the rotation, of the drum.

The resulting hydrazobenzol and-accom-' and heavier liquid content of the charge and the members 12 efiecting in cooperation, upon the rotation'of the drum, a complete agitation of the whole mass of the charge.

The members 12, as shown, are preferably open or perforated intermediately to there by enhance the agitation of the contained charge.

In a commercial embodiment of my invention, the length of the drum may be five feet,

5 the diameter six feet; the radial height of the-shelves not to exceed six inches and the radial'height of the apex of each agitating member not to exceed, two feet.

It will be understood that by the use of the term cylindrical I include all forms of polygonal contour.

By means of my'apparatus the entire zinc content of the charge isrnade available for use as the reaction proceeds, and is also beneficial to man-kind in obviating the dissemination of zinc into the atmosphere and impairing the health of the operator, causing illness and often death, as ensues in the use of .methods and apparatus heretofore employed.

Whereas I have described my invention by reference to specific forms thereof, it will be understood that many changes and modifications may be made without departingfrom the principle of the invention as defined by the appended claims. I claim.

1. The combination with a movable c0n tainer adapted to receivea charge of chemically interacting substances, means for indieating the temperature of the interior of the 1 container. means for elevating within the intenor of the container the relatively heavier substances of the charge and returning the same into the charge comprising a plurality of spaced, relatively narrow shelves disposed within said container, each said shelf extending longitudinally substantially parallel to the direction of length of said container and substantialh continuousl from one end to the other end of saidcontainer, each said shelf having an edge engaging the inner face of said container, each said shelf extending inwardly toward the center of said container,

and spaced agitation members disposed within said container extending inwardly and more closely to the center of the interior of said container than said shelves.

2. The combination-of a substantially, cylindrical container adapted to receive acharge of chemically interaiiting substances; means forindicating exteriorly of the container the temperature of the interior of said container: means for elevating within the interior of said container the relatively heavier substances of the charge and returning the same within. the charge comprising a pluralitvef spaced,

relatively narrow shelves disposed within said container, each said shelf extending longitudinally substantially parallel to the" axis of the sald container and substantially continuously from one end to the other end of said container, each said shelf having an edge engaging the inner cylindrical face of said container, each shelf extending inwardly toward the center of said container; spaced agitation members disposed Within said container extending inwardly and more closely to the center of said container than said shelves and means for moving said bers. r

The combination of a, substantially cylindrical container adapted to receives charge of chemically interacting substances means for indicating extcriorly of said container the temperature of the interior. of said conshelves and said agitation meni-' l tainer; means for elevating within the interior ofsaid container the heavier-substances ofthe charge and returning the same withinthe charge comprisin a plurality of spaced,

the inner cylindrical face of said container;

each. said shelf extending inwardly toward the center of said container and longitudinally substantially continuously from one end'to the other. end 0f said container and substantially parallel to theaxis of said con tainer; spaced agitation members mounted interiorly ofxsaid' container and extending inwardly more-closely toward the'center of said cylinderthan said shelves; and means for rotating said cylinder vand. therewith said shelves and said agitation members.

4;. The combination of -a rotatable cylindrical container having a eharging'iand dischargingopening, liquid-tight closure means for said opening, a plurality of spaced shelves disposed on the inner cylindrical .surfaceofthe container, and means for ro-.

tatin g said container, each said shelf extendinglongitudinally from one end of said container to the other end and inwardly toward the center of said container. 1 5. The combination of a rotc table drical container, having a charging and discharging opening, liquid-tight closure means for said opening, a plurality of spaced shelves disposed" on the inner cylindrical surface of the container, each said shelf extending longitudinally substantially contin uously from one end to the other of said container and substantially parallel to the axis of said container, a'plural-ity of agitation members extending between said shelves and the center of the container and means for rotating said container.

6. The c'ombination of a rotatable cylindrical container having a charging and discharging opening, liquid-tight closure means for, said opening, a plurality of spaced shelves disposed on the inner cylindrical surface of the container, each said shelf extending longitudinally substantially continuously from one end to theother end of said container and substantially parallel to the axis of said container, a plurality of spaced, recessed agitation members extending between said shelves and the center of the container and means for rota-ting said container.

7. The combination of a hollow drum, trunnionscarried at the opposite circular ends of said drum, bearings for said trunnions, one of said trunnions being hollow, a discharge piping in gas-tight relation to said hollow trunnion, said drum having a charging and discharging opening, a liquidtight closure for said opening, spaced shelves disposed on the inner cylindrical surface of heavier tainer, each said I shelfhavin saiddrum and extending radially inwardly and longitudinally of said drum substantially parallel to the axis of theJd'ruIn, re-

cessed agitation members extending from said shelves respectively towards the center of the drum, saidmembers being staggered relatively to one another and'means for rotating said drum. v

-8. The combination of a substantially cylindrical containeradapted to receive a charge of chemically interacting substances; means for'indic'ating exteriorly of said con-- tainer the -temperature of the interior of-said container; means for elevating within the interior of said contalner the relatively substances of the charge and returning the same within the chargecoma plurality of spaced, relatively prising shelves fixed-to the inner cylindrical faceof said container, each said-shelf having a longitudinal edge engaging the inner cylindrical faceof said container; each said shelf extending inwardly toward the center of said container and longitudinally substantially continuously from one end to the other end of said container and substan- 'tially parallel to the axis of said container;

sp'acedagitation members mounted interiorly of and fixed to said container and extending inwardly more closely toward the center of said cylinder than said shelves; and means for rotating said cylinder and therewith said shelves and said agitation members.

9. Thecombination of va substantially cyl indrical' container adapted to receive a charge of chemically interacting substances, one end of said container being provided with an opening, means for rotatablymounting said container, passage means. commn nieating with said opening; means for indicatingexteriorly of said-container a temper-=- ature of the interior of said container; means for elevating within the interior of. said co-ntainerthe relativelyheavier' substances of the charge and returning thesame within the charge comprising relatively narrow shelves extending longitudinally substantially parallel to the axis of said conits outward longitudinal edge fixedto'an engaging the inner face of said container, each said shelf extending toward the center of said container and spaced agitation members respwtively mounted on the inward longitudinal edges of said shelves. 7

10. The combination of a cylindrical container, one end of said container being provided with an opening, means for rotatably mounting said container, passage means communicating with said opening; relatively narrow shelves extending longitudinally substantially parallel to the axis of said container, each said shelf having its outward longitudinal edge fixed to and engaging the inner faceof said container, each said shelf extending toward the center of said container and spaced agitation members respectively mounted on the inward longitudinal edges of said shelves, each said agitation member being interiorly recessed.

11. The combination of a cylindrical container, oneend of said container being provided with an opening, means for rotatably mounting said container, passage means communicating with said opening; relatively narrow shelves extending longitudinally substantially parallel to the axis of said container, each said shelf having its outward longitudinal edge fixed to and engaging the inner face of saidcontainer, each said shelf extending toward the center of said container and spaced agitation members respectively mounted on the inward longitudinal edges of said shelves, said agitation members being disposed in staggered relation toone anothe V 12. The combination of a cylindrical container, one end of said container being provided with an opening, means for rotatably mountin said container, passage means communicating with said opening; relatively narrow shelves extending longitudinally substantially parallel to the axis of said container, each said shelf having its outward longitudinal edge'fixed to and engaging the inner face of said container, each said shelf extending toward the center of said container and spaced agitation members respectively mounted on the inward longitudinal edges of said shelves, said agitation members being interiorly recessed and disposed in staggered relation to one another.

13. The combination with a movable container adapted to receive a charge of solid and liquid constituents, said container be- -in provided with means for retaining the solid and liquid constituents of the charge; means for discharging the gases evolved by chemical action upon movement of the container; said container being further provided with a charging opening and a removable fluid-tight closure for said charging opening; means for elevating within the interior of said container the relatively heavier constituents of the charge and respecification turning the same within the charge com'pris ing a, plurality of spaced, relatively nars row shelves disposed within said container on said shelf extending longitudinally substantially parallel to the direction of length of said container and substantially'contim' uously from one end to the other end of said a container, each said shelf having an edge engaging the inner cylindrical face of said.

container, each said shelf extending in-' wardly toward the center of said container;

spaced agitation members disposed within said container extending inwardly and more closely to the center of said containerthan said shelves and means for moving said shelves and said agitation members.

14. The combination of a substantially terior of said container the relatively heavier constituents and returning the same within the charge comprising a plurality of spaced, relatively narrow shelves fixed'to the inner cylindrical face of said container,each said shelf having a longitudinal edge engaging the inner cylindrical face of said container; each said shelf 7 extending inwardly toward the center of said container and longitudinally substantially continuously from one end-to the other end of said container and substantially parallel to the axis of said container; spaced agitation members mounted interiorly of said container and extending inwardly more closely toward the. center of said cylinder than said shelves; and means for rotating said cylinder and therewith said shelves and said agitation members. 7 v V In testimony whereof I have signed this this 23rd da of May, 1918.

WILLIA H. MAHLER. 

